Potassium Iodide → HCID 69764959, Verbindung

Temperatur

90 °C

3-(4-Hydroxy-phenyl)-acrylic acid hexadecyl ester (4.8 g, 12.4 mmol) was dissolved in 100 ml of NMP. To this was added 6-chlorohexanol (2.19 g, 16 mmol), anhydrous potassium carbonate (1.7 g, 12 mmol) and a catalytic amount of potassium iodide. The reaction was stirred at 90° C. for 18 hours. Water was added to the cooled solution, which was subsequently extracted with 3×100 mls of ethyl acetate. The combined organics were washed with water (2×100 mls), water/brine (100 ml, 50:50) and brine solution and then dried over magnesium sulfate. The concentrated product was purified by silica gel chromatography eluting with 25% ethyl acetate in hexane to give 2.6 g white solid.

1. extractionwas subsequently extracted with 3×100 mls of ethyl acetate
2. washThe combined organics were washed with water (2×100 mls), water/brine (100 ml, 50:50) and brine solution
3. dry with materialdried over magnesium sulfate
4. customThe concentrated product was purified by silica gel chromatography
5. washeluting with 25% ethyl acetate in hexane

ORD-Eintrag

ord-d2c7eaeb460a4023a41f277e9ba3d8ce

Quelldatensatz

uspto-grants-2005_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06919404B2